water separation

Journal Pre-proof Highly efficient and reusable superhydrophobic/superoleophilic polystyrene@ Fe3 O4 nanofiber membrane for high-performance oil/water separation Sara M. Moatmed, Mohamed Hamdy Khedr, S.I. El-dek, Hak-Yong Kim, Ahmed G. El-Deen

PII:

S2213-3437(19)30631-1

DOI:

https://doi.org/10.1016/j.jece.2019.103508

Reference:

JECE 103508

To appear in:

Journal of Environmental Chemical Engineering

Received Date:

15 September 2019

Revised Date:

26 October 2019

Accepted Date:

29 October 2019

Please cite this article as: Moatmed SM, Khedr MH, El-dek SI, Kim H-Yong, El-Deen AG, Highly efficient and reusable superhydrophobic/superoleophilic polystyrene@ Fe3 O4 nanofiber membrane for high-performance oil/water separation, Journal of Environmental Chemical Engineering (2019), doi: https://doi.org/10.1016/j.jece.2019.103508

This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record. This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article. Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain. © 2019 Published by Elsevier.

Highly efficient and reusable superhydrophobic/superoleophilic polystyrene@ Fe3O4 nanofiber membrane for high-performance oil/water separation Sara M. Moatmed a, Mohamed Hamdy Khedr a, S. I. El-dek a, Hak-Yong Kim b, * and Ahmed G. El-Deen c * a

Materials Science and Nanotechnology Department, Faculty of Postgraduate Studies for

b

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Advanced Sciences (PSAS), Beni-Suef University, Beni-Suef 62511, Egypt Department of BIN Convergence Technology, Chonbuk National University, Jeonju 561756,

South Korea

Renewable Energy Science and Engineering Department, Faculty of Postgraduate Studies for

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Advanced Sciences (PSAS), Beni-Suef University, Beni-Suef 62511, Egypt

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* Corresponding authors

E-mail: [email protected] (A.G. El-Deen)

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E-mail: [email protected] (H.Y. Kim)

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Graphical Abstract

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ABSTRACT

Due to increasing of oil spills and high organic contamination of marine environment,

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developing of cost-effective and rapid oil/water separation technique has become inevitable. Herein, freestanding and flexible hybrid polystyrene nanofibers are introduced as highly efficient hybrid membrane for ultrafast oil/water separation without external pressure. Typically, different

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loading of Fe3O4 nanoparticles embedded into polystyrene nanofibers using electrospinning to

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fabricate superhydrophobic/super-oleophilic membrane. The morphological shape, crystal structure and surface wettability behavior were elucidated by field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and contact angel, respectively. The optimum loading of magnetite nanoparticles into the nanofiber membranes was investigated to achieve best separation performance. The obtained results demonstrated that the incorporation of (Fe3O4) nanoparticles into membrane has a significant 2

impact for enhancing superhydrophobic properties and the separation efficiency against light and heavy oils. Among all formulations, the fabricated (PS@Fe3O410wt.%) membrane revealed ultrahigh flux (5000 L.m-2.h-1) with separation efficiency of 99.8% for hexane under gravity driven process and excellent superhydrophobicity with water contact angle 162º moreover excellent reusability 98.5% for 50 consecutive cycles. Interestingly, the proposed hybrid nanofiber membrane achieved distinct separation efficiencies 95% and 92% for food oils such as olive oil

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and sesame oil. Overall, the current study provides cost-effective and facile approach to distinctly

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improve the membrane performance for durable oil/water separation technique.

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Keywords: Superoleophilicity; hybrid nanofiber membrane; Electrospinning; Oil/water

1. Introduction:

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separation.

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Oil spills poses one of the greatest dilemmas faced the global community. Moreover, industrial oily wastewater contamination resulting from different factories such as food, dyes, and

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petrochemical represent the main reason for many serious diseases[1,2].In terms of increasing awareness of marine protection and stringent regulations on industrial wastewater discharge,

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development of rapid and efficient oil/water separation methodologies has become a critical challenge[3–5]. Interestingly, the expulsion of water from fuel oil is very important issue for safety of engines[6]. Unfortunately, conventional oil separation methods such as floatation[7], skimming and ultrasonic have some limitation as high energy consumption, low separation capacity, time consuming and secondary waste moreover couldn’t separate oil water emulsion[8]. However,

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gravity-driven membrane system (GDM) has been recently emerged as promising alternatives purification technique for drinking or rainwater treatment due to no power consumption, low operation and maintenance cost[9–11].Various type polymers have been used as membrane materials including Polyacrylonitrile (PAN), polyvinylidene fluoride (PVDF), polyurethane (PU), polysulfone (PSF) and Polystyrene (PS)[12–16]. Compared to the utilized polymers, PS is widely used in containers for food and drinks moreover introduced as promising membrane materials due

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to its excellent characteristics such as cheap, good chemical inertia, high hydraulic stability, easy to handle and superhydrophobic behaviour[17–19]. To enhance the polymer membrane

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performance, various techniques such as chemical modification[20], surface treatment and blending nanomaterials have been investigated[21–23]. Recently, numerous nanomaterials

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embedded into polymeric matrix as silica nanoparticles (NPs), ZnO NPs, magnetic NPs

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demonstrated improvement in porosity, permeability and separation efficiency of membrane[24– 27].Besides the chemical composition of membrane, fabrication process has significantly impact on

the

membrane

characteristics

including

mechanical

properties,

porosity

and

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permeability[28].Consequently, surface roughness and flexibility play vital role for oil/water separation process, selecting an ideal substrate is also challenge[29,30]. Recently, several oil/water

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separation processes have been reported using simple casting method for fabricating thin film membrane or spray coating substrates as stainless-steel mesh[31,32], copper mesh[33], spongy[34]

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and cotton[35]. However, these strategies still fare from desirable separation capacity and reusability. Among various morphological structures, nanofibers (NFs) have several advantages such as long axial ratio, no agglomeration behavior, free standing and flexible systems shapeable[36]. Electrospinning technique is a facile, efficient, and robust strategy to fabricate different fibers-based nanostructure[37,38]. Electrospun nanofiber membranes have attract great

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deal of attentions in different applications because of good flexibility properties, high specific surface area and uniformly porous structure[39,40]. PS nanofiber coated stainless steel mesh has been introduced as first time for oil/water separation within few minutes using syringe pump[41,42]. Jiang et al. prepared different polymer composite including PAN, PVDF, PS and Fe3O4 as oil sorbents materials boosted magnetic nanoparticles to enhance the oil removal capacity and easy collect from the solution after materials saturated[43,44]. It is worth mentioning that

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surface coated using metal oxides or other functionalized group can enhance the oil/water separation performance[45]. However, the releasing of nanoparticles form of the surface coated

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membrane during process distinctly reduce the performance of membrane[46]. The blending of Fe3O4 NPs with polymer or spongy support materials not only provide significantly increase in the

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separation performance and reusability but also accelerate the diffusion rate of membrane may be

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attributed to oleophilic behaviour, excellent adsorption capacity and magnetic features[47–49]. In this work, a simple strategy is introduced to fabricate robust and effective PS@Fe3O4 nanofiber

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membrane for ultrafast gravity driven oil/water separation. Moreover, the ratio of Fe3O4 nanoparticles in the composite membrane has been optimized to achieve best separation efficiency and the highest flux rate. Interestingly, the flux rate and superhydrophobicity of (PS@Fe3O410%)

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membrane compared to reported materials in the recent nanocomposite membranes.

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2. Experimental 2.1 Materials

Polystyrene (PS) (Mw = 192,000), very fine Fe3O4 nanopowder with ~50nm particle size and nhexane, dimethylformamide (DMF) (99.8%) were provided from Sigma–Aldrich. All chemicals and solvents were used without any further purification.

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Fig. 1. Schematic illustration of the superhydrophobic Fe3O4@PS electrospun nanofiber

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membrane.

2.2 Synthesis of polystyrene nanofibrous membrane

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20g of polystyrene was dissolved in 80 ml of DMF and then stirred for 10 h in water bath at 80ºC to form clear PS solution with 20%. After stirring, the solution was loaded in a syringe of

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10mL volume. The feeding rate of polymer was controlled as 1.2 mL/h using a syringe pump and the distance between the ground collector and the syringe needle was fixed at 18 cm with 18 KV.

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The electrospun nanofiber mats were collected on aluminum foil and dried overnight under vacuum at 60oC.

2.3 Synthesis of Fe3O4 intercalated polystyrene nanofibrous hybrid membrane Different ratio (2%,5%, 10 wt.%) of Fe3O4 were blended respectively to 10 ml of PS solution and stirred for 2h. The polymer matrix solution was transferred to 10 ml of plastic syringe 6

for electrospinning process under same conditions of pristine PS nanofibers. Fig. 1 displays schematic diagram for the fabrication process of freestanding hybrid nanofiber membranes. 2.4 Characterization and measurements The morphologies structures of the Fe3O4@PS electrospun fiber mats were characterized using field emission scanning electron microscopy (FE-SEM Hitachi S- 4700, Japan). The phase

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and crystal structure were characterized using a PANalytical (Empyrean) X-ray diffraction with Cu Kα (λ =1.540°A) radiation, angle range from 10:80° with scan step of 0.04°. Fourier transform

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infrared (FTIR) spectra were analyzed by VERTEX 70/70v spectrometer in the range 400– 4000cm-1. The surface wettability properties of the proposed nanofiber membranes were detected

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using (Ramé-Hart Model 21AC Standard Contact Angle Goniometer/Tensiometer) by sessile-drop

2.5 Separation process

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technique at room temperature.

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To setup the oil/water separation cell, the nanofiber mats with diameter of 10 cm were adjusted between two acrylic cylinders. The mixture solution was prepared by mixing of two equal volume of 50 mL oil and water solution then the mixture poured directly into the acrylic cell, and

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the separation was carried out under gravity without any pressure. The oil flux efficiency for the

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proposed nanofibers mats was recorded and calculated by the following equation (1)[50]:

𝐽𝑤 =

𝑉 𝐴×𝑡

(1)

where 𝐽𝑤 (L.m-2.h-1) is pristine oil flux, V (L) represents the volume of passed oil, A (m2) is the effective area of membrane, and t (h) is the separation time. To evaluate the separation performance for all configuration nanofibers mats, the amount of feed

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and passed oil after separation process was recorded and calculated using the following equation (2)[51]:

𝛾=

𝑚1 𝑚0

× 100%

(2)

where 𝛾 is the separation efficiency, 𝑚1 is the mass of permeate and 𝑚0 presents the mass of feed

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oil during separation process. To investigate the cycling stability of the proposed electrospun nanofiber membranes, the separation process was repeated over 50 cycles. To confirm the accuracy of the reusability test, the

3. Results and discussion

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prepared membrane was dried under vacuum oven at 80 ºC for 2h.

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3.1. Characterization

XRD analysis is very useful technique to determine crystallographic phases of the prepared

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materials. Fig. 2 depicts the XRD patterns for the introduced Fe3O4 NPs and PS@ Fe3O4 nanofiber mats. As shown in this figure, all characteristic peaks of Fe3O4 NPs at 2 = 35.665o, 43.33o and

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62.88o corresponding to the (311), (400) and (440) reflection planes according to the (JCPDS No. 19-629)[52]. The PS@Fe3O4 fibrous composite shows a distinct broad peak related to amorphous polymer and same characteristic peaks of Fe3O4 indicates uniformly distribution of nanoparticles in PS nanofibers. Furthermore, the low intensity and slightly shifted of the diffraction peaks due to amorphous structure of PS matrix. 8

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3.2 Morphological structure

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Fig. 2. XRD pattern of the Fe3O4 NPs and PS@ Fe3O4 10 wt.% nanofiber mats.

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Figure 3a and b shows FESEM and TEM images of the Fe3O4 nanoparticles. Obviously, a uniform distribution of ultrafine Fe3O4 spheres-like structure with average particle size of 50 nm. The

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surface topography and morphology structure for PS electrospun nanofiber and its composite (PS@Fe3O4 10wt.%) were presented in Fig. 4. Obviously, all configuration electrospun nanofibers

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mats show continuous fiber structure without beads or cuts. Fig. 4 (b, c and d) depicts the incorporation of different ratio of (2, 5 and 10 wt.%) Fe3O4 nanoparticles into PS no cracks in nanofibers and uniformly distribution of Fe3O4 NPs into PS NFs. Furthermore, significant decrease in PS fiber diameters were detected with increasing of Fe3O4 NPs content where the average diameters were calculated as 840 nm for pristine PS NFs, 730 nm, 680 and 560 nm for (2, 5 and 10 wt.%) respectively, as shown in Fig. 4(e). It can be attributed to blending of Fe3O4 with 9

polystyrene solution that led to increase the rough surface of membrane, enhance the conductivity of polymer matrix and increase carrying charge during electrospinning process consequently elongating the fiber structure to produce thinner fibers. Fig. 4(e) displays high magnification FESEM image of PS@Fe3O410 wt.%. Surface roughness and porosity of PS NFs with keeping the backbone structures can be observed. Moreover, energy-dispersive X-ray spectroscopy (EDS) in Fig. 4(F) confirmed the chemical composition and demonstrated the existence of Fe, and O

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elements in the characterized area from the center of the membrane and the elemental mapping in

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the inset figure exhibited good and uniformly distribution of the Fe3O4 NPS into PS NFs.

Fig. 3. (a) FESEM image and TEM image (b) of Fe3O4 nanoparticles.

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Fig. 4. FESEM images of (a) pristine PS electrospun nanofiber, Fe3O4 intercalated PS

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nanofibers mats with different ratio (2%, 5% and 10 wt.%) and the inset figure is high magnification of PS @ Fe3O4 10 electrospun mats, (e) the average diameters versus loading Fe3O4 NPs content into PS nanofibers and EDX patterns of PS with Fe3O4 10 wt.%(f) and the inset is elemental mapping.

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Fig. 5(a-d) displays the optical images of the introduced electrospun nanofiber membrane. As shown in Fig. 5 (a), the obtained pristine PS nanofibers membrane was fluffy as cotton-like structure and can't not fixed easily based membrane. A darker colored and robust nanofibers mats were obtained with adding Fe3O4 NPs into PS nanofiber and the color gradually converted from white

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to brown color based on Fe3O4 concentration as shown in (Fig. 5).

Fig. 5. Optical images of the prepared electrospun nanofibers: (a) pristine PS mat, (b) PS/

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Fe3O4 2%, (c) PS@Fe3O4 5% and PS@Fe3O410%(d). 3.3 FTIR spectra of hybrid nanofiber membranes

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Fourier transform infrared spectrometry (FTIR) is widely employed technique to identify

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the functional groups. Fig. 6(a) showed characteristics bands of C-H substituted benzenic ring at 758 cm-1 and 690 cm-1, stretching band of aliphatic saturated C-H at 2850 cm-1, 1610 cm-1 and 1565 cm-1 correspond to C-C bonds of aromatic, and 1158 cm-1 and 1026 cm-1 of aromatic deformation vibration of C-H related to the chemical composition of pure polystyrene nanofiber mat[53]. Fig. 6(b) displayed strong characteristic peaks of Fe3O4 at 580 cm−1 can be attributed to the Fe-O vibration from magnetite lattice and Fe-O stretching vibrations (460 - 628 cm-1)[54,55]. 12

All characteristic peaks of PS and Fe3O4 were observed in fig 6 (c) reflecting successful intercalating of Fe3O4 NPs into PS nanofibers. The low intensity of Fe3O4 peaks with little shift can be

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attributed to blending low amount of Fe3O4 into the PS@ Fe3O4 nanofiber mats.

Fig. 6. FT-IR spectra of different fabricated mats: (a) pure PS NFs, (b) Fe3O4 NPs and PS@ Fe3O4 10 wt.% mats (c).

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3.4 Surface wettability measurements Contact angle measurements proved to be useful and powerful technique to characterize the surface wettability behavior. Fig. 7(a) displays water contact angles (WCA) for the fabricated electrospun nanofibers membranes. Compared to all formulations, PS@Fe3O4 10 wt.% composite achieved higher water contact angles. Typically, the water contact angles were 125 º ,127 º,158 º

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and 162º for pure PS, PS@Fe3O4 (2, 5 and 10 wt.%) respectively. This improvement in superhydrophobicity can be attributed to high surface energy and roughness resulting from Fe3O4 intercalated PS fibers. Optical image in Fig. 7(b) reflects the surface wettability behavior of the electro-

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spun PS@Fe3O4 10 wt.% mats. Clearly, full rejection of water droplets and completely penetration

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of oil droplet with ~0o oil contact angle (OCA) which confirmed the superhydrophobic and super-

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oleophilic surface of hydride PS nanofiber membrane.

Fig. 7. Contact angle of PS and PS@Fe3O4 2%,5%, and 10 wt.% (a) and optical images of surface wettability behavior for the PS@Fe3O4 10% water droplets (right) and commercial oil droplet (left).

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3.5 Separation performance for the proposed nanofiber membrane

Fe3O4 for increasing

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separation rate which PS@Fe3O4 10 wt.% achieved flux efficiency (5000 L.m-2.h-1) around 10 folds compared to pristine PS membrane. To achieve higher accuracy in the separation test, all

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experiments

of oil-in-water via gravity-

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separation

driven

PS@Fe3O4 10wt.% achieved highest separation efficiency over

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99.5%. Interestingly, ultrafast gravity-driven oil/water separation process was observed (video S1, Supporting information). The PS@Fe3O4 10% performed very fast separation of hexane passed

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within only 21 seconds compared to 2.35 minutes for neat PS nanofiber membrane. Cycle lifetime is one of the most requested features to elucidate the cycling stability and

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reusability for materials-based membrane. The reusability test of the prepared PS@Fe3O4 10 wt.% membrane was examined over 50 cycles during membrane process under

. As shown in

Fig. 9(c), the PS@Fe3O4 10wt.% achieved 98.5% in separation retention over 50 cycles; this finding confirms excellent reusability with durable separation efficiency.

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Fig. 8. Optical images of setup oil/water separation process; n-hexane and colorized water

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using methylene blue.

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.

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Fig. 9. Flux efficiency of pure PS and PS@Fe3O4 (2%,5% and10%) composite (a), separation

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efficiency of different samples (b) and cycling stability of PS@Fe3O4 10% membrane(c).

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To ensure the applicability and durability of the fabricated nanofiber membrane, different oils densities including n-hexane, petroleum ether, gasoline oil, olive oil and sesame oil have been applied under gravity driven separation process. As shown in figure 10, The as-prepared PS@Fe3O4 10 wt.% revealed ultrahigh flux for light oils with excellent separation efficiency around 99.8% and even high density of food oils such as sesame oil, the separation efficiency achieved 92%. These results elucidated that the PS@Fe3O4 10 wt.% composite nanofiber poses robust and efficient

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membrane for multi separation process. The prepared PS@Fe3O4 10 wt.% membrane revealed superior water rejection and excellent oleophilic behavior with ultrahigh flux rate of 5000 L.m-2.hcompared to other metal oxides including TiO2, ZnO and recent reported membranes under various

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operating conditions as summarized in table 1.

Fig. 10. Separation efficiency and flux efficiency of PS@Fe3O4 10 wt.% for different oil-water mixtures

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Special wettability

Flux (L.m-2.h-1)

Contact Angle

PVDF membrane/polyamide

Hydrophilic/underwater oleophobic

890

148º OCA

[56]

PDMS/PS

Superhydrophilic/ superoleophobic

4760

162º WCA

[57]

Cellular PAN/SiO2

aerogels/ Superhydrophobic/superoleophilic

1590

PS nanoporous fibersbased sorbents materials Oleophilic/hydrophobic Superhydrophobic/superoleophilic

Aminated PAN-Ag

Superhydrophobic/superoleophilic

PVDF/dopamineAPTES@A-MWCNTs

Superhydrophilicity–underwater superoleophobic

[43]

[60]

oil sorption 130.5º capacity 16.09 WCA g/g 1600 163º OCA

[61]

Superhydrophilic/underwater superoleophobic

8606 under 0.9 155º bar OCA

[23]

Superhydrophobic/superoleophilic

828.95

171º WCA

[63]

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900 under 0.09 153.8º MPa OCA

Superhydrophilicity–underwater superoleophobicity

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[62]

PS@TiO2 (10wt%)

Superhydrophobic/superoleophilic

382

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PVDF/ ZnO

4774.6 +45.6

[42]

[59]

Superhydrophobic–superoleophilic

PVDF/DA@TEOS

[58]

171º WCA

PVDF/CoFe2O4

PAN/HPEI/PDA

162º WCA

oil sorption NA capacity of 113.87 g/g oil sorption 128º capacity 35–45 WCA

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PVDF/Fe3O4@PS composite nanofibers

Ref

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Materials

115 WCA

º This work

PS@ ZnO (10wt%)

Superhydrophobic/superoleophilic

630

120 WCA

º This work

PS @Fe3O4 (10wt%)

Superhydrophobic/superoleophilic

5000

162º WCA

This work

Table. 1. Comparison of flux efficiency for different membrane materials recently published

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Conclusions In conclusion, ultrafast, standalone and superhydrophobic/superoleophilic PS@Fe3O4 electrospun nanofiber hybrid membranes were successfully fabricated via one pot strategy of incorporating ultrafine Fe3O4 nanoparticles into PS electrospun nanofiber using electrospinning. Generally, all PS@Fe3O4 nanofiber composite have high water contact angle and fast oil diffusion

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rate compared to pristine PS nanofiber. However, PS@Fe3O4 having 10wt% achieved excellent separation efficiency of 99.8% and ultrahigh flux-based gravity driven process of (5000 L.m-2.h-1). Furthermore, the prepared PS@Fe3O4 10wt.% membrane exhibits flexible, robust and remarkable

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performance with excellent reusability of membrane can be achieved over 50 cycles without any

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significant decrease. Overall, the proposed study revealed new avenue for using hybrid polystyrene nanofiber membrane as durable and effective approach which meet the requirements for real

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separation process on large scale.

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Declaration of interests

The authors declare that they have no known competing financial interests or personal relationships that

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could have appeared to influence the work reported in this paper.

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The authors declare the following financial interests/personal relationships which may be considered as potential competing interests:

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